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CN102671584B - Reactor and method for preparing particle material - Google Patents

Reactor and method for preparing particle material Download PDF

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CN102671584B
CN102671584B CN201210147355.4A CN201210147355A CN102671584B CN 102671584 B CN102671584 B CN 102671584B CN 201210147355 A CN201210147355 A CN 201210147355A CN 102671584 B CN102671584 B CN 102671584B
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reactor cavity
reactor
granular materials
gas
cavity
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CN102671584A (en
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储晞
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Abstract

The invention discloses a reactor and method for preparing a particle material. The reactor for preparing the particle material comprises more than one reactor cavity body, wherein each reactor cavity body is used for forming and stacking a particle bed layer; the upper end of each reactor cavity body is respectively provided with a first feeding port and a second feeding port; the lower end thereof is correspondingly provided with a first discharging port and a second discharging port; a raw material gas inlet is arranged on the sidewall of the reactor cavity body at one side close to the first feeding port and the first discharging port; a tail gas outlet is arranged on the sidewall of the reactor cavity body at to one side close to the second feeding port and the second discharging port; a first distributor and a second distributor are respectively arranged inside the reactor cavity body to be close to the raw material gas inlet and the tail gas outlet; and each reactor cavity body is externally or internally provided with a dynamic generating mechanism. The invention also discloses a method for preparing the particle material. According to the reactor and method for preparing the particle material, disclosed by the invention, a plurality of disadvantages in the prior art are overcome, and efficient and energy-saving, long-term and steady, safe and reliable preparation of the particle material is realized.

Description

Prepare reactor and the method for granular materials
Technical field
The present invention relates to granular materials technology of preparing, particularly relate to a kind of reactor and the method for preparing granular materials.
Background technology
In modern industry production technology to granular materials as simple substance such as silicon, nickel and titaniums; While the demand of the compounds such as silicon nitride, carborundum and silica is increasing, also more and more harsher to the requirement of its performance: granular materials will meet higher purity requirement; And it is uniform granularity, moderate; The production cost of granular materials is unsuitable too high, to meet the needs of large-scale continuous production.
The first-selected reactor of current production granular materials is fluidized-bed reactor, selected unstrpped gas is adopted (can at high temperature to be decomposed, or reduce, be oxidized, the reaction such as nitrogenize and gas containing target material element in chemical composition) implement the process such as thermal decomposition or reduction, oxidation or nitrogenize in the reactor, the object element simple substance in unstrpped gas is made (to form bed in the reactor in advance at grain seed, and supplement in course of reaction) surface constantly deposits, collected after reaching set particle size, become required granular materials.
The thermal decomposition of above-mentioned raw materials gas is the irreversible reaction process that gas decomposes, and common are:
Thermal decomposition of silane prepares polysilicon; SiH 4---Si+H 2
Carbonyl nickel decomposes nickel processed: Ni (CO) 4---Ni+CO
Etc..
As for raw materials used gas, can be utilize the simple substance element corresponding to target material to be prepared by chemical method, and become the higher unstrpped gas of purity by series of physical and chemical means purifying, belong to the production field of unstrpped gas, what the present invention paid close attention to is utilize these unstrpped gases through effective technical process and controlled condition, and the industrialization for granular materials is produced and provided scientific and effective enforcement technology.
The fluidized-bed process of current employing is produced granular materials and at least be there is following shortcoming:
After unstrpped gas sends into reactor cavity, need by set gas distributor, the yield of unstrpped gas utilization rate and granular product is improved to make unstripped gas as far as possible fully react in reaction chamber, because unstrpped gas is decomposed at any time in reactor cavity, the inlet end of air inlet and gas distributor is caused to form blocking due to particle deposition, need timing cleaning, not only reduce product yield, be also difficult to the needs meeting continuous prodution;
The simple substance that unstrpped gas decomposites in reactor cavity, except being deposited on grain seed surface, also can forming deposition at cavity inner wall, raw material gas inlet and pipeline, while reducing product yield, also affect the long-term continuous and steady operation of fluid bed;
Unstrpped gas is decomposed to form simple substance deposition, while grain seed is grown up, also causes easily being bonded in cavity to be formed between particle reuniting, have impact on the collection of product, breaks in production can only carry out necessary process;
Utilize unstrpped gas to carry out SS during preparation material, air consumption is large, and gas internal circulating load is large, and needing there is a large amount of free space in fluidized-bed reactor cavity, unstrpped gas decompose themselves produces a large amount of dust, is difficult to collect, decrease raw material availability, add cost.
Summary of the invention
The invention provides a kind of reactor preparing granular materials, in order to solve defect of the prior art, realize energy-efficient, steady in a long-term, safe and reliable preparing granular materials.
A kind of reactor preparing granular materials disclosed by the invention, comprise: more than one reactor cavity, described reactor cavity is for the formation of packed particle bed, the filling rate of described granular materials seed is more than 20%, or more than 50%, described filling rate is that in reactor cavity, granular materials seed accounts for the volume for the formation of packed particle bed region in described reactor cavity, described reactor cavity upper end is respectively arranged with the first charge door and the second charge door, and lower end is provided with the first discharging opening and the second discharging opening accordingly; The reactor cavity body sidewall of close first charge door and the first discharging opening side is provided with unstrpped gas entrance, the reactor cavity body sidewall of close second charge door and the second discharging opening side is provided with offgas outlet;
Described reactor cavity is inner is respectively arranged with the first distributor and the second distributor near unstrpped gas entrance with near offgas outlet place, and described first distributor and the second distributor are used for making assist gas and unstrpped gas be scattered in described reactor cavity; The flow direction of the granular materials seed in described assist gas and reactor cavity does not fix requirement, and its flow direction with granular materials seed can be reverse, in the same way or become arbitrarily angled.Unstrpped gas flowing direction can become arbitrarily angled with the flow direction of granular materials seed, preferably vertically;
Described reactor cavity is provided with internal or external dynamic generation mechanism, described dynamic generation mechanism is kept in motion for making the packed particle material bed being positioned at described reactor cavity, namely be in relative motion state between adjacent granular materials seed, with avoid mutual bonding thus affect course of reaction continue carry out;
Described reactor lower part is provided with grain products discharging opening and solid circle discharging opening, described solid circle discharging opening is connected with particle transport mechanism, the granular materials being positioned at reactor cavity lower end can be delivered to reactor cavity upper end by described particle transport mechanism, granular materials seed in packed particle material bed is kept in motion, avoids the bonding between granular materials seed.
Further, described reactor comprises reactor cavity described in two or more, contacted by the first discharging opening of upper level reactor cavity and the first charge door of next stage reactor cavity between each reactor cavity, the second discharging opening of upper level reactor cavity is contacted with the second charge door of next stage reactor cavity and realizes connecting; As N stage reactor cavity is connected with N+1 stage reactor cavity, be connected with N+1 level first charge door by the first discharging opening of N level; Be connected with N+1 level second charge door by N level second discharging opening; The reactor cavity of series connection can make realize Multiple depositions by the granular materials seed of its inside and constantly grow up;
Reactor cavity described in chopped-off head is provided with internal or external preheating mechanism;
Described grain products discharging opening and solid circle discharging opening are all positioned at final stage reactor cavity bottom.
Further, realize described series connection between adjacent two-stage reactor cavity by bringing-up section, described bringing-up section and the conducting of described adjacent two-stage reactor cavity, described bringing-up section can be external or be built-in with the pipeline of heater.
Further, the join domain between described adjacent two-stage reactor cavity forms reducing.Namely higher level's discharging opening is undergauge, and subordinate's charging aperture is expanding, is beneficial to and eliminates intergranular bonding and reunion, and make to keep relative motion because being squeezed between particle.
Further, described reactor cavity body sidewall is also provided with assist gas charge door, for carrying assist gas in reactor, described assist gas can be used for dilution unstrpped gas, stirring packed particle bed prevents unstrpped gas entrance and reactor cavity inwall sedimentation of solid material with anti-caking, generation gas curtain.
Further, described reactor cavity is provided with internal or external heating arrangements, this heating arrangements can provide the heating of different temperatures to the zones of different of the packed particle bed in reaction cavity, raise from the temperature between the first distributor to the second distributor to meet packed particle bed.
Further, described heating arrangements is built-in heating arrangements, at least comprises one of following mechanism: be arranged at the heater in described reactor cavity, for heating the packed particle bed formed; Inside be provided with the heat exchanger tube of thermal source (as combustion heating, eddy-current heating, resistance heated or heating using microwave), described heat exchanger tube is arranged in described reactor cavity, and is located in reactor cavity body sidewall; When the granular materials forming packed particle bed is conductive material, the power supply be electrically connected with the described first or second packed particle material bed, the first or second packed particle material bed flows through the resistance heated self formed by electric current.
When described heating arrangements is external heating arrangements, heat autoreactor cavity wall is externally to diffusion inside.
Further, described dynamic generation mechanism is unstrpped gas nozzle and/or gas assist nozzle, describedly be arranged in described reactor cavity, be connected with unstrpped gas entrance and/or the auxiliary gas entry be arranged on reactor cavity body sidewall respectively, unstrpped gas and/or assist gas to be spurted in described reactor cavity from least one unstrpped gas nozzle and/or gas assist nozzle in the mode of continuous or pulse and are stirred packed particle material bed; Or
Described dynamic generation mechanism is the particle transport mechanism that the granular materials being positioned at reactor cavity lower end can be delivered to reactor cavity upper end, described particle transport mechanism feed end is connected with solid circle discharging opening, and described particle transport mechanism discharge end is connected with the first and second charge doors; Or
The reducing that join domain between adjacent two-stage reactor cavity is formed, granular materials is keeping relative motion by being squeezed during reducing, namely connect the import of two reactor cavities and outlet is less than reactor cavity internal diameter, have when granular materials flows through two reactor cavities a cross section large-cross section is little-the large process in cross section; Or
For being placed in comb structure in reactor cavity body sidewall or bringing-up section sidewall or heating element heater itself, when granular materials flows through these mechanisms, disperse because of the stop of comb structure to conciliate group.Also gear sub-agencies can be set adding on reactor cavity body sidewall, altering reactor diameter and change the flow direction of granular materials in reactor cavity.
Further, described particulate transportation mechanism is mechanical lifting mechanism or pneumatic conveying mechanism, and described mechanical lifting mechanism is bucket elevator, screw rod hoister or vibrations elevator; Described pneumatic conveying mechanism is that dense phase gas moves conveying equipment, dilute-phase pneumatic conveying equipment, venturi pneumatic conveying equipment or Pneumatic vacuum conveying equipment.
Described bucket elevator comprises: topple over hopper, lower guide channel and upper rail, describedly topple over hopper can travel to and fro between reactor top and bottom by lifting means, described topple over when hopper is positioned at reactor upper end be communicated with the first and second charge doors by upper rail, described in topple over when hopper is positioned at reactor lower end and be communicated with solid circle discharging opening by lower guide channel.Described particulate transportation also comprises and is not limited to following method: screw rod conveyor, vibrations elevator, dense phase gas move conveying equipment, dilute-phase pneumatic conveying equipment, venturi pneumatic conveying equipment or Pneumatic vacuum conveying equipment.
Further, described reactor cavity is provided with internal or external preheating mechanism, for entering the unstrpped gas of reactor cavity, assist gas carries out and/or the preheating of granular materials seed.Described preheating mechanism be by containing the tail gas had surplus heat (or granular materials) be about to add the unstrpped gas of reaction chamber, assist gas and/or granular materials seed and carry out heat exchange, to make full use of residual heat of reaction, reduce energy consumption.
Further, described reactor cavity outer setting has the gas solid separation mechanism be connected with described preheating mechanism, described gas solid separation mechanism for separating of with the dusty material collected in reaction end gas.The dusty material of described gas solid separation collect can be injected in reactor cavity granular materials seed as a supplement, thus effectively utilizes raw material, reduces preparation cost.
Further, described gas solid separation mechanism is the granular materials bed of dense accumulation, and the filling rate of the granular materials bed of described dense accumulation is more than 20%, or more than 50%.
Further, bottom described reactor cavity, be provided with solid circle discharging opening, its first charging aperture by pipeline and reactor cavity and/or the second charging aperture conducting.
Further, described reactor cavity outer setting has tail gas processing mechanism, is connected between described preheating mechanism and described unstrpped gas entrance, for separating of active ingredient in tail gas.
Further, described reactor also comprises internal or external surface trimming mechanism and screening mechanism; Described surface trimming mechanism is used for carrying out surface treatment to the granular materials prepared, and described surface trimming mechanism is the reaction cavity of the unstrpped gas being 0-10% containing concentration.When not containing unstrpped gas in reaction cavity (unstrpped gas containing 0%), each granular materials first product, by phase mutual friction, makes its surface become bright and clean; When containing unstrpped gas in reaction cavity, except the phase mutual friction between each granular materials first product, at granular materials first product surface deposition after the unstrpped gas decomposition of low concentration, granular materials first product surface is made to become bright and clean further; Surface treated granular materials cools collecting packing or is delivered directly to downstream prepares workshop section; Described screening mechanism is connected between described reactor cavity and described surface trimming mechanism, in order to select the granular materials reaching dimensional requirement.Also comprise and being connected for the pulveriser that the granular materials sieved out is carried out pulverizing with described screening mechanism.
Further, described reactor cavity also comprises the air curtain mechanism of the iris action that can provide between reaction mass and reactor cavity inwall;
Described air curtain mechanism is the multiple blow vents be arranged on reactor cavity inwall, especially be located at the multiple blow vents on the reactor cavity body sidewall not having unstrpped gas entrance, offgas outlet and distributor region, and the set-up mode of the plurality of blow vent can make the assist gas passed into form gas curtain along reactor cavity inwall; Or
Described air curtain mechanism is be arranged on the ring pipe around cavity inner wall in reactor cavity, especially the ring pipe in the reactor cavity not having unstrpped gas entrance, offgas outlet and distributor region is located at, described ring pipe communicates with secondary gas source, described ring pipe is provided with multiple gas outlet, when the set-up mode of described gas outlet can make assist gas spray, forms gas curtain along reaction cavity inwall.
In reactor cavity if any position by granular materials flowing serious wear time, unstrpped gas can be supplemented and offset the loss brought by wearing and tearing to allow abrading section be deposited.
Further, described reactor cavity inwall adopts identical with prepared granular materials or makes the material that granular materials does not produce pollution.Such as produce polycrystalline silicon material and at high temperature diffusion impurity can not enter material in reactor cavity with HIGH-PURITY SILICON, high-purity silicon carbide, high purity silicon nitride, quartz or graphite etc.Can reduce or avoid reactor cavity material to the pollution of granular materials.
Further, the height of described reactor cavity is more than 0.1 meter; Or the height of described reactor is more than 0.5 meter.The height of described reactor cavity is 0.1-10 rice; Or the height of described reactor is 0.1-100 rice.
Further, a described reactor cavity forms first order reaction, and the order of reaction of described reactor is 1-50 level; Or be 1-20 level.
The above-mentioned reactor preparing granular materials prepares polysilicon or carbonyl nickel thermal decomposition nickel for thermal decomposition of silane.When being appreciated that other adopt irreversible chemical reaction and physical process to prepare granular materials, also this reactor can be adopted.
The reactor preparing granular materials in the present invention is called for short reactor.
Another object of the present invention discloses a kind of method preparing granular materials, and adopt above-mentioned reactor to realize, described method comprises the steps:
In reactor cavity, granular materials seed is added by the first charge door and the second charge door, form the first packed particle material bed in parallel and second and pile up a material grain bed, and described first packed particle material bed and the second granular materials seed filling rate of piling up in a material grain bed are more than 20%, or more than 50%;
Heat described first and second packed particle material beds, make the temperature of described first packed particle material bed lower than the temperature needed for reaction, and described second packed particle material bed reaches temperature needed for reaction to meet physical-chemical reaction;
Pass into unstrpped gas and necessary assist gas (high-purity H 2and/or inert gas etc. does not participate in reacting gas), make described unstrpped gas after unstrpped gas entrance passes into, can substantially react completely in the first distributor, the first packed particle material bed (low-temperature region) and the second packed particle material bed (high-temperature area) process successively, granular materials seed deposits, and the tail gas formed is by being discharged by offgas outlet after the second distributor; Reacting gas is when by the first distributor, because the first packed particle material bed does not reach reaction temperature, all do not have deposition of material above it, and start when reacting gas enters into the second packed particle material bed to decompose, substantially reacted completely before arrival second distributor, it is inner that the namely decomposition of unstripped gas just occurs in the second packed particle bed.Can prevent or reduce a place in reactor cavity inside, unstrpped gas entrance and gas distributor or many places over-deposit results in blockage, reach long-time continuous stable operation;
Supplement granular materials seed, maintain the dynamic equilibrium of described first and second packed particle material beds, and contact with unstrpped gas cross-flow when making supplemented granular materials seed descending; Described granular materials seed can be purchase granular materials, isolate dusty material in reaction end gas, the size of being sent back to by particle transport mechanism do not meet the requirements of granular materials or the granular materials after pulverizing;
The granular materials seed in described granular materials bed is made to be in relative motion state, and descending through the first and second discharging openings in the reaction;
From in the granular materials first product of the first and second discharging openings, meet the requirements of granular materials first product to discharge from grain products discharging opening, do not meet the requirements of granular materials first product through solid circle discharging opening by described particle transport mechanism Returning reactor cavity granular materials seed as a supplement;
Order between above steps does not limit.
Further, described reactor comprises reactor cavity described in two or more, contacted by the first discharging opening of upper level reactor cavity and the first charge door of next stage reactor cavity between each reactor cavity, the second discharging opening of upper level reactor cavity is contacted with the second charge door of next stage reactor cavity and realizes connecting;
Reactor cavity described in chopped-off head is provided with internal or external preheating mechanism;
Described grain products discharging opening and solid circle discharging opening are all positioned at final stage reactor cavity bottom;
Described method comprises:
In course of reaction, to the first and second packed particle material bed heating in every A reactor cavity, and all pass into unstrpped gas;
Make the granular materials seed of the first and second packed particle material beds of upper level reaction cavity fall into the first and second packed particle material beds of next stage reaction cavity respectively through the first and second discharging opening correspondences, continue granular materials seed is grown up;
Granular materials first product from final stage reactor cavity is discharged from particulate product outlet port, obtains described granular materials.
Further, between the adjacent two-stage reactor cavity of described reactor, realize described series connection by bringing-up section, described bringing-up section and the conducting of described adjacent two-stage reactor cavity; Described method comprises:
The granular materials seed from upper level reaction cavity is made to fall into next stage reactor cavity after described bringing-up section is heated.
Further, the join domain between described adjacent two-stage reactor cavity forms reducing, makes the granular materials seed from upper level reaction cavity pass through the join domain of this reducing and form motion state.
Further, the heating arrangements of described reactor is built-in heating arrangements, at least comprises one of following mechanism:
Be arranged at the heater of described reaction zone, for heating the packed particle bed formed;
Inside be provided with the heat exchanger tube of thermal source, described heat exchanger tube is arranged at described reaction zone, and is located in reactor cavity body sidewall, and keeps sealing with the first or second packed particle material bed;
When described granular materials is conductive material, the power supply be electrically connected with the described first or second packed particle material bed, the resistance heated of the material bed laminar flow of the first or second packed particle through self being formed;
Described method also comprises: utilize described built-in heating arrangements to heat the first and second formed packed particle beds, to make passed into unstrpped gas generation decomposition reaction.
When described heating arrangements is external heating arrangements, heating means are by the diffusion of reactor cavity body sidewall ecto-entad by heat.
Further, the method making the granular materials seed in described granular materials bed be in relative motion state comprises:
Assist gas and/or unstrpped gas are spurted in reactor cavity and stirs granular materials bed; Or
Adopt reducing reactor cavity and change the speed of supplementing granular materials seed and control the time of staying of granular materials seed in reactor cavity; Or
Introduce external force and carry out cross-current comb structure that is spouted, that rotate, stir, mix, vibrate or make granular materials seed to flow through under gravity reactor cavity inwall is installed.
Further, also comprise: from described reaction end gas, isolate dusty material, described dusty material is added described first packed particle material bed and/or second and pile up a material grain bed; Or
The granular materials that part obtains is burst into small-particulate materials, sends described first packed particle material bed and/or second back to and pile up a material grain bed.
Further, the described process isolating dusty material from described reaction end gas is specially: make described reaction end gas through having the gas solid separation mechanism of the granular materials bed of dense accumulation, collect dusty material, the filling rate of the granular materials bed of described dense accumulation is more than 50%.
Further, the granular materials first product also comprised obtaining carries out surface-treated process: by the reaction cavity of described granular materials first product through containing concentration being the unstrpped gas of 0-10%.Decompose deposition of particulate material surface by friction and low concentration unstrpped gas and obtain the granular materials of any surface finish.
Further, correspond to product particle discharge outlet in described reactor cavity and is also provided with screening mechanism, bottom described reactor cavity, be provided with solid circle discharging opening, its first charging aperture by pipeline and described reactor cavity and/or the second charging aperture conducting; Described method also comprises:
Carry out screening process to the granular materials first product obtained, the granular materials first product that size does not reach regulation is discharged from solid circle discharging opening, and participates in reaction in granular materials seed Returning reactor cavity as a supplement.Also comprise: the granular materials bulky grain prepared is obtained even-grained granular materials product through screening.
Further, in course of reaction, make reactor cavity inwall form gas curtain by air curtain mechanism, the air curtain mechanism of described reactor is:
Be arranged on the multiple blow vents on reactor cavity inwall, and the set-up mode of the plurality of blow vent can make the assist gas passed into form gas curtain along reactor cavity inwall; Or
Described air curtain mechanism is be arranged on the ring pipe around cavity inner wall in reactor cavity, described ring pipe communicates with secondary gas source, described ring pipe is provided with multiple gas outlet, when the set-up mode of described gas outlet can make assist gas spray, forms gas curtain along reaction cavity inwall;
The method of described formation gas curtain is, in reactor cavity, assist gas is passed into by described air curtain mechanism, make assist gas in reactor cavity along inwall flowing, realize the obstruct of granular materials first product to obtained and reactor cavity inwall and/or unstrpped gas and reactor cavity inwall.
Described granular materials is the simple substance that can exist alone under nature or the compound (as nitride, carbide, oxide or sulfide) containing these simple substance, or a kind of below: the nitride of germanium simple substance, carbon simple substance, elementary silicon, nickel simple substance, titanium simple substance, carborundum, silica, nickel, the carbide of nickel, the nitride of titanium, the carbide of titanium.
Described assist gas is inert gas or the gas not participating in reaction.
Described unstrpped gas is: the compound containing target material and/or can be oxidized with it, reduce, the gas of the chemical reaction such as carbonization or nitridation reaction; Described target material and granular materials.
Further, the temperature needed for described reaction is 100-3000 ° of C, and the pressure in reactor cavity is 0.001-100MPa.Compared with producing granular materials with existing fluidized-bed process, the present invention has following several respects advantage:
When unstrpped gas is by reactor cavity, first carry out preheating through the first granular materials bed that excess temperature is lower, reach through excess temperature higher (reaching decomposition temperature) second granular materials bed again and decompose substantially completely, prevent or reduce the deposition of product on distributor, simultaneously, owing to introducing and reactor cavity inwall and tangent shielding gas flow, make the operation of reactor continous-stable;
In the present invention, reactor cavity is provided with particle transport mechanism and the granular materials being positioned at reactor cavity lower end is delivered to reactor cavity upper end, drive stratum granulosum moves, without the need to gas suspension, operation does not affect by flow of feed gas, assist gas is for diluting unstrpped gas, producing gas curtain or stir particle layers, air consumption is little, and gas internal circulating load is little;
In the present invention, reactor cavity is provided with particle transport mechanism, granular materials seed in packed particle material bed is kept in motion, avoids the bonding between granular materials seed, reduce reactor volume.In addition the join domain between adjacent two-stage reactor cavity forms reducing, also can reduce the bonding between granular materials seed further;
And by the high-purity powder silicon in the granular materials bed capture reaction tail gas of dense accumulation as seed, also utilize the waste heat of reaction end gas to be supplementary granular materials heating;
This invention takes closs packing and move bed, the space in reactor cavity is less.The generation of dust and overflow less, adds the utilization rate of raw material, reduces operating cost, and make practical operation safe and reliable;
To sum up, present invention achieves efficient, energy-conservation, continuous, low cost long-time continuous stable and prepare granular materials.
Accompanying drawing explanation
The structure of reactor schematic diagram preparing granular materials that Fig. 1 provides for embodiment one;
Fig. 2 is particle transport mechanism structure schematic diagram;
Fig. 3 a, Fig. 3 b are the structural representation of reactor cavity gas curtain;
Fig. 3 c, Fig. 3 d are the structural representation of unstrpped gas pipeline gas curtain;
The structure of reactor schematic diagram preparing granular materials that Fig. 4 provides for embodiment two.
Detailed description of the invention
Embodiment one
The structure of reactor schematic diagram preparing granular materials that Fig. 1 provides for embodiment one; Fig. 2 is particle transport mechanism structure schematic diagram; Fig. 3 a, Fig. 3 b are the structural representation of reactor cavity gas curtain; Fig. 3 c, Fig. 3 d are the structural representation of unstrpped gas pipeline gas curtain;
As shown in Figure 1, the reactor of what the present embodiment provided prepare granular materials, comprising: two-stage reactor cavity, two-stage reactor cavity forms two-stage reaction, and the height of reactor cavity is 0.5 meter, and the height of reactor is 1.5 meters.
Reactor cavity is for the formation of packed particle bed, the filling rate of granular materials seed is more than 50%, first reactor cavity upper end is respectively arranged with the first charge door 101a and the second charge door 101b, and lower end is provided with the first discharging opening 102a and the second discharging opening 102b accordingly; Be realize series connection in the following manner between the two-stage reactor cavity preparing granular materials: the first discharging opening 102a of first order reactor cavity is contacted by the first bringing-up section 110a with the first charge door of second level reactor cavity, the second discharging opening 102b of first order reactor cavity and the second charge door of second level reactor cavity pass through the second bringing-up section 110b and contact; Bringing-up section can be external or be built-in with the pipeline of heater.The two-stage reactor cavity of series connection can make realize twice deposition by the granular materials seed of its inside and grow up; In addition, multistage reactor cavity can make by parallel connection and increase production capacity;
The reactor cavity body sidewall of close first charge door 101a and the first discharging opening 102a side is provided with unstrpped gas entrance 115, the reactor cavity body sidewall of close second charge door 101b and the second discharging opening 102b side is provided with offgas outlet 116;
Reactor cavity is inner is respectively arranged with the first distributor 112a and the second distributor 112b near unstrpped gas entrance 115 with near offgas outlet 116 place, and the first distributor 112a and the second distributor 112b is used for making assist gas and unstrpped gas be scattered in reactor cavity; The flow direction of the granular materials seed in assist gas and reactor cavity does not fix requirement, can be reverse, in the same way or become arbitrarily angled with the flow direction of granular materials seed.The flow direction of unstrpped gas flowing granular materials seed is vertical.
Reactor cavity is provided with built-in dynamic generation mechanism, and dynamic generation mechanism is kept in motion for making the packed particle material bed being positioned at reactor cavity; Dynamic apparatus in this reactor comprises: the reducing that the join domain between two-stage reactor cavity is formed.Namely higher level's discharging opening is undergauge, and subordinate's charging aperture is expanding, is beneficial to and eliminates intergranular bonding and reunion, and make to keep relative motion because being squeezed between particle; In addition, unstrpped gas nozzle and gas assist nozzle is also provided with in reactor cavity, be connected with the auxiliary gas entry be arranged on reactor cavity body sidewall with unstrpped gas entrance respectively, unstrpped gas and assist gas to be spurted in reactor cavity from unstrpped gas nozzle and gas assist nozzle in the mode of continuous or pulse and are stirred packed particle material bed;
The reactor cavity bottom, the second level of reactor is provided with grain products discharging opening and solid circle discharging opening, solid circle discharging opening is connected with particle transport mechanism, the granular materials being positioned at reactor cavity lower end can be delivered to reactor cavity upper end by particle transport mechanism, granular materials seed in packed particle material bed is kept in motion, avoids the bonding between granular materials seed.
Concrete particulate transportation mechanism (bucket elevator) comprises as shown in Figure 2: topple over hopper 1, lower guide channel 2 and upper rail 3, topple over hopper 1 can travel to and fro between reactor top and bottom by lifting means, topple over when hopper 1 is positioned at reactor upper end and be communicated with the first and second charge doors by upper rail 3, topple over when hopper 1 is positioned at reactor cavity lower end and be communicated with solid circle discharging opening by lower guide channel 2.In the present invention, transporting of granular materials seed is not limited to gas, and adopts mechanical system, so reaction has a larger operating space.Screw rod conveyor, vibrations elevator, dense phase gas can be selected in addition to move conveying equipment, dilute-phase pneumatic conveying equipment, venturi pneumatic conveying equipment or Pneumatic vacuum conveying equipment.
First order reactor cavity first charge door and the second charge door are provided with external preheating mechanism; For to entering the unstrpped gas of reactor cavity, assist gas carries out and/or the preheating of granular materials seed.Preheating mechanism be by containing the tail gas had surplus heat (or granular materials) be about to add the unstrpped gas of reaction chamber, assist gas and/or granular materials seed and carry out heat exchange, to make full use of residual heat of reaction, reduce energy consumption.
In order to make active ingredient in tail gas can be separated rear further and recycle, reactor cavity outer setting has tail gas processing mechanism, is connected between preheating mechanism and unstrpped gas entrance, for separating of active ingredient in tail gas.
Reactor cavity body sidewall is also provided with assist gas charge door, for carrying assist gas in reactor, assist gas can be used for dilution unstrpped gas, stirring packed particle bed prevents unstrpped gas entrance and reactor cavity inwall sedimentation of solid material with anti-caking and generation gas curtain.
Reactor cavity is provided with built-in heating arrangements, be arranged at the heater in reactor cavity, for heating the packed particle bed formed, this heating arrangements can provide the heating of different temperatures to the zones of different of the packed particle bed in reaction cavity, raise from the temperature between the first distributor 112a to the second distributor 112b to meet packed particle bed.
Reactor cavity outer setting has the gas solid separation mechanism be connected with preheating mechanism, gas solid separation mechanism for separating of with the dusty material collected in reaction end gas.Gas solid separation mechanism is the granular materials bed of dense accumulation, and the filling rate of the granular materials bed of dense accumulation is more than 50%.The dusty material of gas solid separation collect can be injected in reactor cavity granular materials seed as a supplement, thus effectively utilizes raw material, reduces preparation cost.
Reactor also comprises internal or external surface trimming mechanism and screening mechanism; Surface trimming mechanism is used for carrying out surface treatment to the granular materials prepared, and surface trimming mechanism is the reaction cavity of the unstrpped gas being 0-10% containing concentration.Surface treated granular materials cools collecting packing or is delivered directly to downstream prepares workshop section; Screening mechanism is connected between reactor cavity and surface trimming mechanism, in order to select the granular materials reaching dimensional requirement.Also comprise and being connected for the pulveriser that the granular materials sieved out is carried out pulverizing with screening mechanism.
Reactor cavity also comprises the air curtain mechanism of the iris action that can provide between reaction mass and reactor cavity inwall; As shown in Figure 3 b, air curtain mechanism is be arranged on the multiple blow vents on the reactor cavity body sidewall not having unstrpped gas entrance, offgas outlet and distributor region, and the set-up mode of the plurality of blow vent can make the assist gas passed into form gas curtain along reactor cavity inwall; Or for being arranged on the ring pipe in the reactor cavity not having unstrpped gas entrance, offgas outlet and distributor region, ring pipe communicates with secondary gas source, ring pipe is provided with multiple gas outlet, when the set-up mode of gas outlet can make assist gas spray, forms gas curtain along reaction cavity inwall.Air curtain mechanism as shown in Fig. 3 a, Fig. 3 c and Fig. 3 d can also be adopted to prevent connecting line, unstrpped gas entrance, offgas outlet and reactor cavity inwall deposition materials further.Air curtain mechanism shown in Fig. 3 a is at unstrpped gas entrance or for the reactor cavity inwall near its outlet arranges blow vent, allows assist gas form the gas curtain along the flowing of reactor cavity inwall by passage; Air curtain mechanism shown in Fig. 3 c and Fig. 3 d is: unstrpped gas air inlet pipe is provided with passage, in raw material air inlet pipeline, assist gas (single arrow) is passed into by passage, allow assist gas mode that is parallel along pipeline or spiral flow, unstrpped gas (double-head arrow) and pipeline inner wall are separated.
In reactor cavity if any position by granular materials flowing serious wear time, unstrpped gas can be supplemented and offset the loss brought by wearing and tearing to allow abrading section be deposited.
Reactor cavity inwall adopts HIGH-PURITY SILICON to make, and is appreciated that the material that do not produce pollution to silicon grain material such as high-purity silicon carbide, high purity silicon nitride, quartz or graphite etc. at high temperature all diffusion impurity can not enter material in reactor cavity.Can reduce or avoid reactor cavity material to the pollution of granular materials.
The above-mentioned reactor preparing granular materials prepares polysilicon or carbonyl nickel thermal decomposition nickel for thermal decomposition of silane.When being appreciated that other adopt irreversible chemical reaction and physical process to prepare granular materials, also this reactor can be adopted.
Generate polysilicon for silane pyrolysis below, describe the method preparing silicon grain in detail, step is as follows:
In reactor cavity, granular materials seed (polysilicon seed) is added by the first charge door and the second charge door, form the first packed particle material bed in parallel and second and pile up a material grain bed, and described first packed particle material bed and the second granular materials seed filling rate of piling up in a material grain bed are more than 50%;
Utilize built-in heating arrangements to heat the first and second packed particle material beds of two-stage reactor cavity simultaneously, make the temperature of described first packed particle material bed lower than the temperature needed for reaction, temperature is 300-400 degree, and described second packed particle material bed reaches temperature needed for reaction to meet physical-chemical reaction, temperature is 650-800;
Pass into unstrpped gas (silane) and necessary assist gas (H to connecting in a reactor cavity simultaneously 2), make described unstrpped gas after unstrpped gas entrance passes into, can substantially react completely in the first distributor, the first packed particle material bed (low-temperature region) and the second packed particle material bed (high-temperature area) process successively, granular materials seed deposits, and the tail gas formed is by being discharged by offgas outlet after the second distributor; Reacting gas is when by the first distributor, because the first packed particle material bed does not reach reaction temperature, so there is no deposition of material above it, and start when reacting gas enters into the second packed particle material bed to decompose, substantially reacted completely before arrival second distributor, it is inner that the namely decomposition of unstripped gas just occurs in the second packed particle bed.Can prevent or reduce a place in reactor cavity inside, unstrpped gas entrance and gas distributor or many places over-deposit results in blockage, reach long-time continuous stable operation;
Make the granular materials seed of the first and second packed particle material beds of first order reaction cavity respectively through the first and second discharging openings, corresponding the first and second packed particle material beds falling into second level reaction cavity of the first and second bringing-up sections, continue granular materials seed is grown up;
Make the granular materials seed in described granular materials bed be in the method for relative motion state as follows: the join domain between two-stage reactor cavity forms reducing, make from first order reaction cavity granular materials seed through this reducing join domain and form motion state.Assist gas and unstrpped gas are spurted in reactor cavity simultaneously and stir granular materials bed.
Granular materials first product from second level reactor cavity is discharged from particulate product outlet port, obtains described granular materials.
Supplement granular materials seed, maintain the dynamic equilibrium of described first and second packed particle material beds, and contact with unstrpped gas cross-flow when making supplemented granular materials seed descending; Described granular materials seed can be that granular materials, isolated dusty material in reaction end gas, the size of being sent back to by particle transport mechanism purchased does not meet the requirements of granular materials or the granular materials after pulverizing.
The granular materials seed in described granular materials bed is made to be in relative motion state, and descending through the first and second discharging openings in the reaction.
The job step of particle transport mechanism is: be arranged in reactor cavity lower end do not arrive product size require granular materials flow into dumpable hopper 1 by solid circle discharging opening by the guiding of lower guide channel 2, after dumpable hopper 1 is filled, lower guide channel 2 is closed, do not arrive the granular materials stopping flowing that product size requires, dumpable hopper 1 is thus lifted to the upper end of reactor cavity, upper rail 3 is opened, and with dumpable hopper 1 UNICOM, granular materials in dumpable hopper 1 guides the first charge door and the second charge door that flow into first order reactor cavity through upper rail 3, enter reactor cavity, granular materials seed in reactor cavity from top to bottom moves under gravity, the granular materials seed in the first and second packed particle material beds is kept to be in relative motion state, also the effect of dynamic generation mechanism can be played.After granular materials in dumpable hopper 1 empties, the lower end of Returning reactor cavity and lower guide channel 2 UNICOM, again feed, then repeat above-mentioned action again.It should be noted that the conveying of whole granular materials should at H 2or carry out under the atmosphere of inert gas, in order to avoid high-temperature particle material is polluted by other gases (as chlorine) and reduces quality.
Above-mentioned particle transport mechanism is the comparatively economic method of a particle carrying.Conventional fluidization bed utilizes unstrpped gas to carry out suspended particle material seed when producing material, needs a large amount of air supporting, and usual fluid bed needs a minimum fluidizing velocity Umf to maintain operation.And carry out moving particles material seed by the method for machinery in the present embodiment, and do not rely on gas.The flow of assist gas and unstrpped gas is not by the minimum restriction of floating flow velocity of conventional fluidization bed, and air-flow can be less than critical fludization velocity air velocity and can control between 0.01Umf-10Umf.Following benefit can be brought thus: save air-flow, reduce heating and energy loss, reduce vent gas treatment amount, decreasing pollution; Make of the present invention when producing opereating specification large, gas is the amount doesn't matter, can not stop production because of the interim minimizing of raw material.
In addition, the method making the granular materials seed in described packed particle bed be in relative motion state also comprises: 1) spurt in reactor cavity by assist gas and/or unstrpped gas, and packed particle bed is kept in motion; 2) introduce external force carry out as spouted, rotate, stir, mix, vibrate or the cross-current comb structure of gravity current downflow by reactor cavity inwall is installed; 3) under making reactor be in other gravitational fields (as centrifugal force field etc.); 4) agitated bed is used; 5) vibrated bed (comprising mechanical oscillation, sound wave or ultrasonic wave vibration, plug-in type vibrating etc.) is used; 6) adopt reducing reactor cavity and change the speed of supplementing granular materials seed and control the time of staying of granular materials seed in reactor cavity.
The granular materials first product of the first and second discharging openings from second level reactor cavity is carried out screening process, meeting the requirements of granular materials first product can directly discharge from grain products discharging opening.But the present embodiment is in order to improve granular materials quality, also the granular materials first product that size reaches regulation is obtained to screening and carrying out surface treatment: by the reaction cavity of described granular materials first product through containing concentration being the unstrpped gas of 0-10%.Decompose deposition of particulate material surface by friction and low concentration unstrpped gas and obtain the granular materials of any surface finish.The unstrpped gas that concentration is lower carries out dense coating to granular material surface, thus makes the surface-brightening of each granular materials clean and tidy.Produce after the granular materials that obtains carries out surface treatment, enter cooler and cool through inert gas, last collecting packing or be delivered directly to downstream production workshop section.
Screening process does not meet the requirements of granular materials first product through solid circle discharging opening by particle transport mechanism Returning reactor cavity granular materials seed as a supplement; From reaction end gas, isolate dusty material, by dusty material also as a supplement granular materials seed add the first packed particle material bed and second pile up a material grain bed; The process isolating dusty material from reaction end gas is specially: make described reaction end gas through having the gas solid separation mechanism of the granular materials bed of dense accumulation, collect dusty material, the filling rate of the granular materials bed of described dense accumulation is more than 50%.This process not only can prevent dusty material from entering reaction downstream, and can simple, free of contamination generation granular materials seed.Also can be separated by gas componant isolating the reaction end gas after dusty material, isolated assist gas being transmitted back in reactor cavity and recycling.Also using tail gas as the thermal source in preheating mechanism, heat exchange can be carried out with granular materials seed, unstrpped gas or assist gas.
The size that granular materials seed in the present embodiment is mainly derived from reactor lower end solid circle discharging opening does not reach isolated dusty material in the granular materials of standard and tail gas.When granular materials seed source is not enough, the granular materials that part obtains is burst into small-particulate materials granular materials seed as a supplement, send the first packed particle material bed and/or second back to and pile up a material grain bed.Also comprise, by screening process, the granular materials bulky grain prepared is obtained even-grained granular materials product through screening.
Order between above steps does not limit.
In course of reaction, reactor cavity inwall is made to form gas curtain by air curtain mechanism, the method of described formation gas curtain is, in reactor cavity, assist gas is passed into by described air curtain mechanism, make assist gas in reactor cavity along inwall flowing, realize the obstruct of granular materials first product to obtained and reactor cavity inwall and/or unstrpped gas and reactor cavity inwall.
Assist gas is H 2; Granular materials is silicon, and unstripped gas is silane.Reaction pressure in reactor cavity is 0.1-100 atmospheric pressure, preferably 0.1-50 atmospheric pressure.
Embodiment two
The structure of reactor schematic diagram preparing granular materials that Fig. 4 provides for embodiment two.
Be appreciated that the first and second charge doors described in embodiment one, the first and second granular materials beds, the first and second discharging openings etc. are all a kind of extreme cases arranged for the ease of understanding, but not limitation of the present invention.In fact, as long as unstrpped gas is not reacted when entering particle layers, and complete reaction is just passable when leaving particle layers, and without the need to being deliberately divided into two-way, concrete just can be able to be realized by the setting of the heating power in portion each in stratum granulosum.
As shown in Figure 4, the reactor preparing granular materials disclosed in the present embodiment comprises: reactor cavity, and described reactor cavity is for the formation of packed particle bed, and the filling rate of granular materials seed is more than 20%;
Described reactor cavity upper end is provided with charge door 201, and lower end is provided with discharging opening accordingly;
The upper end of the lower end packed particle bed of charge door is provided with heating arrangements 203, heating arrangements 203 is five heat exchanger tubes be arranged in parallel, be provided with thermal source in described heat exchanger tube, described thermal source is the electrically heated rod of 1.0KW, and five heat exchanger tubes to be located in reactor cavity body sidewall and to be connected with power supply; And heat exchanger tube and the unstrpped gas flow direction in reactor cavity is vertical arranges.
After two heat exchanger tubes series connection of unstrpped gas entrance, then with other three in parallel, the heat exchanger tubes of two series connection are the first heating system, and other three is the second heating system, and the heating power of the first heating system is lower than the heating power of the second heating system.
On the reactor cavity body sidewall of the first heating system, be also provided with unstrpped gas entrance 205, on the reactor cavity body sidewall of the second heating system, be also provided with offgas outlet 204;
Reactor cavity is inner is also respectively arranged with the first distributor 206 and the second distributor 207 near unstrpped gas entrance 205 with near offgas outlet 204 place; Heating arrangements 203 can provide the heating of different temperatures to the zones of different of the packed particle bed in reaction cavity, raise from the temperature between the first distributor to the second distributor to meet packed particle bed.
Reactor cavity is provided with built-in dynamic generation mechanism, and dynamic generation mechanism is kept in motion for making the packed particle material bed being positioned at described reactor cavity;
Reactor lower part is provided with grain products discharging opening 202 and solid circle discharging opening, described solid circle discharging opening is connected with particle transport mechanism 208, and the granular materials being positioned at reactor cavity lower end can be delivered to the charge door 201 of reactor cavity upper end by particle transport mechanism 208.Particle transport mechanism is pneumatic transporting equipment.
Adopt above-mentioned reactor, the method for polysilicon prepared by thermal decomposition of silane, comprise the following steps:
In reactor cavity, add granular materials seed (silicon grain material) by charge door 201, form the packed particle material bed that filling rate is more than 20%.
The material bed laminar flow of described packed particle is through heating arrangements, packed particle material bed near the first heating system is the first packed particle material bed, first packed particle material bed is heated to 300-400 degree, temperature is lower than the temperature needed for silane decomposes, and be the second packed particle material bed near the packed particle material bed of the second heating system, second packed particle material bed is heated to 650-800 degree, and temperature meets silane decomposes temperature;
Pass into unstrpped gas SiH 4with assist gas argon gas, wherein SiH 4account for 40% of total tolerance, make unstrpped gas after unstrpped gas entrance passes into, can substantially react completely in the first distributor, the first packed particle material bed and the second packed particle material bed process successively, granular materials seed deposits, and the tail gas formed is by being discharged by offgas outlet after the second distributor;
Supplement granular materials seed, maintain the dynamic equilibrium of described first and second packed particle material beds, and contact with unstrpped gas cross-flow when making supplemented granular materials seed descending;
The granular materials seed in described granular materials bed is made to be in relative motion state, and descending through discharging opening in the reaction;
From in the particle of discharging opening, meet the requirements of granular materials first product and discharge from grain products discharging opening 202, obtain finished silicon granular materials.Do not meet the requirements of granular materials first product through solid circle discharging opening by particle transport mechanism 208 Returning reactor cavity granular materials seed as a supplement;
Order between above steps does not limit.
Last it is noted that above embodiment is only in order to illustrate technical scheme of the present invention, be not intended to limit; Although with reference to previous embodiment to invention has been detailed description, those of ordinary skill in the art is to be understood that: it still can be modified to the technical scheme described in foregoing embodiments, or carries out equivalent replacement to wherein portion of techniques feature; And these amendments or replacement, do not make the essence of appropriate technical solution depart from the spirit and scope of various embodiments of the present invention technical scheme.

Claims (30)

1. prepare the reactor of granular materials for one kind, comprise: more than one reactor cavity, described reactor cavity is for the formation of packed particle bed, described reactor cavity upper end is respectively arranged with the first charge door and/or the second charge door, and lower end is provided with the first discharging opening and/or the second discharging opening accordingly; The reactor cavity body sidewall of close first charge door and the first discharging opening side is provided with unstrpped gas entrance, and/or the reactor cavity body sidewall of close second charge door and the second discharging opening side is provided with offgas outlet;
Described reactor cavity is inner is respectively arranged with the first distributor and the second distributor near unstrpped gas entrance with near offgas outlet place;
Described reactor cavity is provided with internal or external heating arrangements, this heating arrangements can provide the heating of different temperatures to the zones of different of the packed particle bed in reaction cavity, with meet packed particle bed from described first distributor to described second distributor between temperature raise;
Described reactor cavity is provided with built-in dynamic generation mechanism, and described dynamic generation mechanism is kept in motion for making the packed particle material bed being positioned at described reactor cavity;
Described reactor lower part is provided with grain products discharging opening and solid circle discharging opening, and described solid circle discharging opening is connected with particle transport mechanism, and the granular materials being positioned at reactor cavity lower end can be delivered to reactor cavity upper end by described particle transport mechanism.
2. reactor according to claim 1, it is characterized in that, described reactor comprises reactor cavity described in two or more, contacted by the first discharging opening of upper level reactor cavity and the first charge door of next stage reactor cavity between each reactor cavity, and/or the second discharging opening of upper level reactor cavity is contacted with the second charge door of next stage reactor cavity and realizes connecting;
Reactor cavity described in chopped-off head is provided with internal or external preheating mechanism;
Described grain products discharging opening and solid circle discharging opening are all positioned at final stage reactor cavity bottom.
3. reactor according to claim 2, is characterized in that, realize described series connection between adjacent two-stage reactor cavity by bringing-up section, described bringing-up section and the conducting of described adjacent two-stage reactor cavity.
4. reactor according to Claims 2 or 3, is characterized in that, the join domain between adjacent two-stage reactor cavity forms reducing.
5. reactor according to claim 1 or 2, is characterized in that, described heating arrangements is built-in heating arrangements, at least comprises one of following mechanism:
Be arranged at the heater in described reactor cavity, for heating the packed particle bed formed;
Inside be provided with the heat exchanger tube of thermal source, described heat exchanger tube is arranged in described reactor cavity, and is located in reactor cavity body sidewall;
When the granular materials forming packed particle bed is conductive material, the power supply be electrically connected with the first or second packed particle material bed.
6. reactor according to claim 1 or 2, it is characterized in that, described dynamic generation mechanism is unstrpped gas nozzle and/or gas assist nozzle, described unstrpped gas nozzle and/or gas assist nozzle are arranged in described reactor cavity, are connected respectively with unstrpped gas entrance and/or the auxiliary gas entry be arranged on reactor cavity body sidewall.
7. reactor according to claim 1 or 2, is characterized in that, described reactor cavity is provided with internal or external preheating mechanism, for entering the unstrpped gas of reactor cavity, assist gas carries out and/or the preheating of granular materials seed.
8. reactor according to claim 7, it is characterized in that, described reactor cavity outer setting has the gas solid separation mechanism be connected with described preheating mechanism, described gas solid separation mechanism for separating of with the dusty material collected in reaction end gas.
9. reactor according to claim 8, it is characterized in that, described gas solid separation mechanism is the granular materials bed of dense accumulation, and the filling rate of the granular materials bed of described dense accumulation is more than 20%.
10. reactor according to claim 1 or 2, is characterized in that, is provided with solid circle discharging opening bottom described reactor cavity, its first charging aperture by pipeline and reactor cavity and/or the second charging aperture conducting.
11. reactors according to claim 10, it is characterized in that, described reactor cavity outer setting has tail gas processing mechanism, is connected between preheating mechanism and described unstrpped gas entrance.
12. according to claim 1 or 2 reactor, it is characterized in that, described reactor also comprises internal or external surface trimming mechanism and screening mechanism; Described surface trimming mechanism is used for carrying out surface treatment to the granular materials prepared; Described screening mechanism is connected between described reactor cavity and described surface trimming mechanism.
13., according to reactor described in claim 12, is characterized in that, described surface trimming mechanism is the reaction cavity of the low concentration unstrpped gas being 0-10% containing concentration.
14. according to claim 1 or 2 reactor, it is characterized in that, described reactor cavity also comprises the air curtain mechanism of the iris action that can provide between reaction mass and reactor cavity inwall;
Described air curtain mechanism is the multiple blow vents be arranged on reactor cavity inwall, and the set-up mode of the plurality of blow vent can make the assist gas passed into form gas curtain along reactor cavity inwall; Or
Described air curtain mechanism is be arranged on the ring pipe around cavity inner wall in reactor cavity, described ring pipe communicates with secondary gas source, described ring pipe is provided with multiple gas outlet, when the set-up mode of described gas outlet can make assist gas spray, forms gas curtain along reaction cavity inwall.
15. according to claim 1 or 2 reactor, it is characterized in that, described reactor cavity inwall adopts the material identical with prepared granular materials to make.
16. reactors according to claim 1, it is characterized in that, the height of described reactor cavity is more than 0.1 meter; Or the height of described reactor is more than 0.5 meter.
17. 1 kinds of methods preparing granular materials, is characterized in that, adopt reactor described in claim 1-16 any one to realize, described method comprises the steps:
In reactor cavity, granular materials seed is added by the first charge door and/or the second charge door, form the first packed particle material bed in parallel and second and pile up a material grain bed, and described first packed particle material bed and the second granular materials seed filling rate of piling up in a material grain bed are more than 20%;
Heat described first and second packed particle material beds, make the temperature of described first packed particle material bed lower than the temperature needed for reaction, and described second packed particle material bed reaches the temperature needed for reaction;
Pass into unstrpped gas and necessary assist gas, make described unstrpped gas after unstrpped gas entrance passes into, can substantially react completely in the first distributor, the first packed particle material bed and the second packed particle material bed process successively, granular materials seed deposits, and the tail gas formed is by being discharged by offgas outlet after the second distributor;
Supplement granular materials seed, maintain the dynamic equilibrium of described first and second packed particle material beds, and contact with unstrpped gas cross-flow when making supplemented granular materials seed descending;
The granular materials seed in described granular materials bed is made to be in relative motion state, and descending through the first and/or second discharging opening in the reaction;
In granular materials first product from the first and/or second discharging opening, meet the requirements of granular materials first product to discharge from grain products discharging opening, do not meet the requirements of granular materials first product through solid circle discharging opening by described particle transport mechanism Returning reactor cavity granular materials seed as a supplement;
Order between above steps does not limit.
18. according to method described in claim 17, it is characterized in that, described reactor comprises reactor cavity described in two or more, contacted by the first discharging opening of upper level reactor cavity and the first charge door of next stage reactor cavity between each reactor cavity, and/or the second discharging opening of upper level reactor cavity is contacted with the second charge door of next stage reactor cavity and realizes connecting;
Reactor cavity described in chopped-off head is provided with internal or external preheating mechanism;
Described grain products discharging opening and solid circle discharging opening are all positioned at final stage reactor cavity bottom;
Described method comprises:
In course of reaction, to the first and second packed particle material bed heating in every A reactor cavity, and all pass into unstrpped gas;
Make the granular materials seed of the first and second packed particle material beds of upper level reaction cavity fall into the first and second packed particle material beds of next stage reaction cavity respectively through the first and/or second discharging opening correspondence, continue granular materials seed is grown up;
Granular materials first product from final stage reactor cavity is discharged from particulate product outlet port, obtains described granular materials.
19., according to method described in claim 18, is characterized in that, realize described series connection between the adjacent two-stage reactor cavity of described reactor by bringing-up section, described bringing-up section and the conducting of described adjacent two-stage reactor cavity; Described method comprises:
The granular materials seed from upper level reaction cavity is made to fall into next stage reactor cavity after described bringing-up section is heated.
20., according to method described in claim 18, is characterized in that, the join domain between described adjacent two-stage reactor cavity forms reducing, make the granular materials seed from upper level reaction cavity pass through the join domain of this reducing and form motion state.
21., according to method described in claim 18, is characterized in that, the heating arrangements of described reactor is built-in heating arrangements, at least comprises one of following mechanism:
Be arranged at the heater of reaction zone, for heating the packed particle bed formed;
Inside be provided with the heat exchanger tube of thermal source, described heat exchanger tube is arranged at described reaction zone, and is located in reactor cavity body sidewall;
When described granular materials is conductive material, the power supply be electrically connected with the described first or second packed particle material bed;
Described method also comprises: utilize described built-in heating arrangements to heat the first and second formed packed particle beds, to make passed into unstrpped gas generation decomposition reaction.
22., according to method described in claim 18, is characterized in that, the method making the granular materials seed in described granular materials bed be in relative motion state comprises:
Assist gas and/or unstrpped gas are spurted in reactor cavity and stirs granular materials bed; Or
Adopt reducing reactor cavity and change the speed of supplementing granular materials seed and control the time of staying of granular materials seed in reactor cavity; Or
Introduce external force and carry out cross-current comb structure that is spouted, that rotate, stir, mix, vibrate or make granular materials seed to flow through under gravity reactor cavity inwall is installed.
23., according to method described in claim 18, is characterized in that, also comprise: from reaction end gas, isolate dusty material, described dusty material are added described first packed particle material bed and/or second and pile up a material grain bed; Or
The granular materials that part obtains is burst into small-particulate materials, sends described first packed particle material bed and/or second back to and pile up a material grain bed.
24. according to method described in claim 23, it is characterized in that, the described process isolating dusty material from described reaction end gas is specially: make described reaction end gas through having the gas solid separation mechanism of the granular materials bed of dense accumulation, collect dusty material, the filling rate of the granular materials bed of described dense accumulation is more than 20%.
25., according to method described in claim 18, is characterized in that, the granular materials first product also comprised obtaining carries out surface-treated process: by the reaction cavity of described granular materials first product through containing concentration being the unstrpped gas of 0-10%.
26. according to method described in claim 18, it is characterized in that, correspond to product particle discharge outlet in described reactor cavity and be also provided with screening mechanism, solid circle discharging opening is provided with, its first charging aperture by pipeline and described reactor cavity and/or the second charging aperture conducting bottom described reactor cavity; Described method also comprises:
Carry out screening process to the granular materials first product obtained, the granular materials first product that size does not reach regulation is discharged from solid circle discharging opening, and participates in reaction in granular materials seed Returning reactor cavity as a supplement.
27., according to method described in claim 18, is characterized in that, in course of reaction, make reactor cavity inwall form gas curtain by air curtain mechanism, the air curtain mechanism of described reactor is:
Be arranged on the multiple blow vents on reactor cavity inwall, and the set-up mode of the plurality of blow vent can make the assist gas passed into form gas curtain along reactor cavity inwall; Or
Described air curtain mechanism is be arranged on the ring pipe around cavity inner wall in reactor cavity, described ring pipe communicates with secondary gas source, described ring pipe is provided with multiple gas outlet, when the set-up mode of described gas outlet can make assist gas spray, forms gas curtain along reaction cavity inwall;
The method of described formation gas curtain is, in reactor cavity, assist gas is passed into by described air curtain mechanism, make assist gas in reactor cavity along inwall flowing, realize the obstruct of granular materials first product to obtained and reactor cavity inwall and/or unstrpped gas and reactor cavity inwall.
28. according to any one of claim 17-27 method, it is characterized in that, described assist gas is inert gas or the gas not participating in reaction; Described unstrpped gas is: the compound containing target material and/or can be oxidized with it, reduce, the gas of carbonization or nitridation reaction; Described granular materials is the simple substance that can exist alone under nature or the compound containing these simple substance.
29. according to any one of claim 17-27 method, it is characterized in that, described granular materials is following one: the nitride of germanium simple substance, carbon simple substance, elementary silicon, nickel simple substance, titanium simple substance, carborundum, silica, nickel, the carbide of nickel, the nitride of titanium, the carbide of titanium.
30., according to method described in claim 17, is characterized in that, the temperature needed for described reaction is 100-3000 DEG C, and the pressure in reactor cavity is 0.001-100MPa.
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